Search NASA⌕ Search

SEARCH · Search NASA

Results for “AM Powder Characterization”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 973 records · Page 54
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

High-fraction brookite films from amorphous precursors

Structure-specific synthesis processes are of key importance to the growth of polymorphic functional compounds such as TiO 2 , where material properties strongly depend on structure as well as chemistry. The robust growth of the brookite polymorph of TiO 2 , a promising photocatalyst, has been difficult in both powder and thin-film forms due to the disparity of reported synthesis techniques, their highly specific nature, and lack of mechanistic understanding. In this work, we report the growth of high-fraction (~95%) brookite thin films prepared by annealing amorphous titania precursor films deposited by pulsed laser deposition. We characterize the crystallization process, eliminating the previously suggested roles of substrate templating and Na helper ions in driving brookite formation. Instead, we link phase selection directly to film thickness, offering a novel, generalizable route to brookite growth that does not rely on the presence of extraneous elements or particular lattice-matched substrates. In addition to providing a new synthesis route to brookite thin films, our results take a step towards resolving the problem of phase selection in TiO 2 growth, contributing to the further development of this promising functional material.

14 SOLAR ENERGY↗
DOE OSTI2023

Evidence of plasma‐driven decomposition of common plastics exposed to an atmospheric nonthermal discharge

Abstract A nonthermal, pulsed spark discharge is applied to three polymer powders in Ar and Ar– gas mixtures. Hydrogen is introduced to assess plasma‐driven decomposition. Gaseous decomposition products, including methane, acetylene, and ethylene, are observed with Fourier‐transform infrared (FTIR). Surface modifications are observed on the residual polymer via attenuated total internal reflection‐FTIR. Time‐averaged rotational, vibrational, and excitation temperatures are characterized in the discharge. The plasma density is found to be around , with rotational and vibrational temperatures ranging from 1500 to 2200 K and an excitation temperature of 1–2 eV. While spark properties did not change with either gas composition or polymer composition, it was determined that the addition of hydrogen promoted higher concentrations of gaseous phase products (promoting hydrogenolysis).

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructural evolution in Cu-Nb processed via friction consolidation

Immiscible alloys, whether in well-mixed or layered forms, are of increasing interest based on their novel structural and functional properties, such as enhanced thermal stability against grain growth or radiation-induced defect trapping at the interfaces. To address the need for new approaches to tailor microstructures, the microstructural development of an immiscible Cu-Nb alloy processed via friction consolidation of elemental powders is investigated. Friction consolidation is a solid-phase processing technique that imparts severe plastic strain into a deforming volume resulting in elevated temperatures below the melting temperature of the alloy. Two distinct processing pathways were chosen to understand the effect of thermomechanical conditions on the final microstructure. The microstructure was characterized using scanning electron microscopy, scanning transmission electron microscopy, and X-ray diffraction techniques. Path 1 exhibited larger strain, strain rate, and temperature as compared with path 2. In path 1, agglomerated Nb particles were present in the recrystallized ultrafine-grained Cu matrix, while in path 2 extremely fine and dispersed Nb particles were present in a highly deformed Cu matrix. In both pathways, supersaturation of Cu in Nb lattices was noted, but not vice-versa. The asymmetry in mixing is explained based on deformation-based, thermodynamic and kinetic factors. These findings provide a pathway for creation of novel tailored microstructures and improved properties in any number of binary immiscible alloy systems.

Cu-Nb alloys, Microstructural refinement, Friction↗
DOE OSTI2018

Synthesis and Characterization of Ni{sub 1−x}Cu{sub x}Bi{sub 3} Superconductor

In this paper, we characterized the microstructure and superconducting properties of Cu-doped NiBi{sub 3} samples. The polycrystalline Ni{sub 1−x}Cu{sub x}Bi{sub 3} (0 ≤ x ≤ 0.10) samples were prepared using a solid-state reaction method. The crystal structure and unit cell parameters were determined by Rietveld refinement of powder X-ray diffraction. The data showed that the main phase present corresponded to NiBi{sub 3} without dependence on the Cu concentration, but with small quantities of Ni and Bi. The SEM and AFM measurements revealed that the main phase was inhomogeneous at microscopic level, with Bi richer regions in comparison to other regions. However, Raman spectroscopy results did not show significant changes in the spectra with Cu doping and in different regions of the samples. Another finding was that regardless of Cu doping, the superconducting transition temperature was 4.05–4.06 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Effects of Mg Substitution on the Structural and Magnetic Properties of Ni{sub 0.2}Mg{sub x}Co{sub 0.8−x}Fe{sub 2}O{sub 4} Nanoparticle Ferrites

Sol-gel auto-combustion is a method of preparing ferrite by combining combustion with chemical gel. In this study, Ni-Mg-Co ferrite powders are prepared by coprecipitation method, and the nanocrystals of Ni{sub 0.2}Mg{sub x}Co{sub 0.8−x}Fe{sub 2}O{sub 4} are successfully synthesized. The structure and magnetic properties of undoped and Mg-substituted Ni-Co ferrite nanoparticles are systematically investigated. The methods used to characterize the prepared samples are X-ray diffraction (XRD) analysis, Fourier transform infrared spectroscopy (FTIR), and Vibrating sample magnetometry (VSM). The synthesized samples are confirmed by XRD analysis to form a single-phase cubic spinel structure with crystals between 48 and 50 nm. With the increase of Mg ion concentration, the lattice constant decreases. The results of FTIR spectroscopy indicated that a spinel structure was formed. Transmission electron microscopy (TEM) images show spherical cubic microcrystals in the samples. EDX analysis confirms that the synthesized ferrite is pure phase structure, and Mg{sup 2+} is successfully replaced. With the increase of Mg{sup 2+} ion content, the saturation magnetization and remanent magnetization decreased from 70.16 to 39.77 emu/g and 36.40 to 20.20 emu/g at room temperature, respectively. Meanwhile, the coercivity decreases from 1032.16 to 378.50 Oe by increasing Mg{sup 2+} concentration. This also indicates that the Mg-substituted Ni-Co nano-ferrite has a low magnetic of multi-ferric material. The increasing of peak height of dM/dH at H{sub m} indicates that the cubic spinel structure sample has good crystallinity and magnetic stability.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2022

Comparative investigation of Ga- and In-CHA in the non-oxidative ethane dehydrogenation reaction

Ga- and In-exchanged chabazite (CHA) zeolites with same Si/Al and metal/Al ratios were prepared via the incipient wetness impregnation method, were characterized using N 2 adsorption, electron microscopy, temperature-programed reactions and were evaluated for the ethane dehydrogenation reaction using flow microreactors. Ga-CHA has higher reaction rates and a lower activation energy of 107 kJ/mol than In-CHA (E a = 175 kJ/mol). Rietveld refinement of the X-ray powder diffraction pattern shows that the In + cation is predominantly located above the 6-ring of the CHA cage. It is proposed that the reaction proceeds through the alkyl mechanism based on stability of alkyl hydride intermediates as determined using DFT calculations. The oxidative addition of ethane to the metal shows much lower Gibbs free energy for Ga-CHA (+27.95 kJ/mol) vs In-CHA (+124.85 kJ/mol). Finally, these results indicate that oxidative addition may be the rate-limiting step of ethane dehydrogenation in these materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Gas-Phase Composition as a Predictive Metric for Calendar Life Behavior of Next-Generation Silicon Anodes

The expansion of renewable technologies and electrification of the transportation sector is driving increased demand for next-generation battery materials that provide higher power and energy density with superior cycling and calendar life stability. Silicon (Si) has a theoretical capacity nearly 10x that of graphite, and is therefore a promising anode material candidate to meet these rigorous performance demands. While leading Si anode battery demonstrations are approaching target metrics for cycle life, a series of complex and interrelated modes of reactivity lead to reduced calendar life and therefore challenge practical adoption of these materials. Deconvoluting the degradation processes that impact Si calendar life is critical to informing the rational and accelerated design of improved Si materials. In the present work, we employ novel sampling techniques and GC-MS-FID characterization to measure gas-phase composition during initial Si cycling, which we tie to selective mechanisms of Si passivation. We utilize a tiered analysis approach to identify and quantify the gas-phase reaction products associated with three advanced Si material candidates under practical operating conditions. Ex situ analysis of Si powders (pure chemical reactivity) is coupled with nondestructive in situ sampling of Si electrodes in a practical pouch-cell format (coupled chemical and electrochemical reactivity). We link the observed gas-phase species evolution to electrochemical behavior and measured calendar life of the three Si materials. Further, we evaluate the voltage-resolved evolution of gas-phase species for one such Si nanomaterial, where nonmonotonic gas generation implies competition between passivating reaction pathways. The measured gas-phase compositional data serves as a critical input for our advanced electrochemical SEI models to identify favorable vs unfavorable reaction pathways to stabilize Si. In addition to bolstering a fundamental understanding of Si reactivity, the present approach informs specific and quantifiable gas-phase metrics tied to calendar life improvements in Si, which can streamline and accelerate the process of next-generation material development.

DIRECT ENERGY CONVERSION,ENERGY STORAGE↗
DOE OSTI2025

Laser Powder Directed Energy Deposition of Steels for Nuclear Applications

This comprehensive investigation examines the structure–property relationships in two nuclear alloy systems—Alloy 709 (A709) austenitic stainless steel and Grade 92 (G-92) ferritic/martensitic (F/M) steel—manufactured via directed energy deposition (DED) for sodium-cooled fast reactor applications. This study establishes the fundamental mechanisms for controlling microstructures for optimizing the mechanical performance of additively manufactured nuclear materials through systematic heat treatment optimization and multiscale characterization. As-deposited A709 steel develops a complex multiscale strengthening architecture consisting of a fine cellular solidification structure with diameter of 2-3 µm within10–50 µm grains, elevated dislocation densities from rapid thermal cycling, and grain boundary precipitates that activate concurrent Hall–Petch, dislocation, and precipitation hardening mechanisms to achieve exceptional properties [yield strength (YS): 603 MPa, ultimate tensile strength (UTS): 844 MPa, Vickers hardness: 220 HV] that achieve a 44% superior strength compared to that of the wrought material. Heat treatments produce different results. Solution annealing (SA) dissolves the cellular structure and reduces the hardness to 190 HV. Precipitation treatment (PT) keeps the cellular structure but adds carbides, allowing the hardness to reach 205 HV. The best approach combines both treatments (SA+PT) and creates uniform precipitate distributions with M 23 C 6 carbides at the grain boundaries and MX carbonitrides in the matrix, achieving a hardness of 195 HV. However, directional differences persist, with a 12%–15% strength variation between orientations due to the inherited layered microstructural architecture that survives aggressive heat treatment. While tensile testing at 550°C demonstrates 40%–50% thermal softening with dynamic strain aging, DED A709 steel still maintains a 71% higher YS than that of the wrought material. Ion irradiation studies (100–400 dpa) of DED A709 steel reveal progressive radiation damage with increasing void density and radiation-induced segregation causing nickel enrichment and chromium depletion, which will ultimately compromise mechanical properties. As-deposited G-92 exhibits exceptional strength (UTS: 1650–1700 MPa, 430 HV) through a complex microstructure containing both ferrite and martensite phases, a high geometrically necessary dislocation (GND) density (17.04×10 14 /m 2 ), and fine carbides. Heat treatments create distinct changes. Normalizing produces fresh martensite with the highest hardness (460 HV) and an increased GND density (20.23×10 14 /m 2 ). Tempering develops dual precipitation systems and reduces the hardness to 290 HV. The optimal approach uses sequential normalizing plus tempering, achieving balanced properties with the lowest hardness (250 HV) and a reduced GND density (11.01×10 14 /m 2 ). A processing-dependent anisotropy is observed: horizontal specimens achieve superior ductile behavior, while vertical specimens exhibit brittle failure. A tempering heat treatment successfully mitigates this anisotropic behavior by transforming the hard martensitic as-deposited structure into tempered martensite enabling both horizontal and vertical specimens to exhibit similar stress–strain characteristics with visible necking behavior. Remarkably, testing at 550°C reveals a reversal in the anisotropy, where as-deposited specimens achieve near isotropy with superior thermal stability (a 15%–20% strength reduction), while tempered specimens develop an orientation dependence with a 25%–30% strength reduction. Both alloy systems demonstrate that DED processing creates specimens with a superior strength through refined microstructural features, though with distinct strengthening mechanisms—austenitic through cellular structures and precipitates versus F/M through phase transformations and precipitates. Heat treatment optimization requires alloy-specific approaches, with A709 benefiting from controlled precipitation while G-92 requires careful phase transformation control. The results show that DED manufacturing can produce nuclear materials with exceptional performance, but directional effects and temperature-dependent behavior must be carefully considered for reactor component design and qualification.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2018

Effects of carbon content and size on Ti-C reaction behavior and resultant properties of Cu-Ti-C alloy system

Highlights: • TiC-strengthened Cu alloys were synthesized by an in situ powder metallurgy route. • Effect of C/Ti ratio on electrical and mechanical properties was studied. • Ti-C reaction behavior during powder metallurgy process was discussed. • Microstructure evolution during present process was analyzed. - Abstract: TiC-strengthened Cu alloys with various nominal compositions were prepared by a high-energy ball-milling process, followed by consolidation using spark plasma sintering (SPS), and a subsequent heat treatment. The results indicated that the lower atomic ratio of C/Ti, the more residual Ti in copper matrix, resulting in a lower electrical conductivity but higher microhardness of alloy. The optimal atomic ratio was found to be close to1.0. The reaction behavior of Ti-C in the Cu-Ti-C system during this process was investigated. Microstructural results suggested that TiC formation is through a diffusion-controlled mechanism. A thin TiC layer was formed at the surface of C particles, and the growth of TiC layer was controlled by interdiffusion of C and Ti atoms across the TiC layer. An incomplete chemical reaction between Ti and C, characterized by a core-shell structure, was observed when the initial C particles were large, and the TiC particle size was found to strongly depending on the C particle size.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Preliminary Feasibility of Printing, Microstructure Analysis and Mechanical Performance of a Down Selected Ni Alloy

This report is submitted as completion of a Milestone 3 deliverable under work package ORNL CT-23OR1304051 in support of the Advanced Materials and Manufacturing Technologies (AMMT) program. The AMMT program is aiming at the faster incorporation of new materials and manufacturing technologies into complex nuclear-related systems. An integrated approach, combining advanced characterization, high-throughput and accelerated testing, modeling and simulation including machine learning and artificial intelligence will be employed. While 316H (Fe-16-18Cr-10-14Ni-2-3Mo-0.04-0.1C) has been identified as a key alloy to be integrated into the AMMT accelerated alloy qualification approach due its relevance for many current and future nuclear energy reactors, many other alloys could be considered for the advanced fabrication of innovate high-performance nuclear components. ANL, INL, ORNL and PNNL are collaborating on identifying the most promising alloy candidates relevant for the AMMT program. A selection criteria matrix was established to evaluate the alloys considering their relative importance and technological readiness levels for nuclear energy applications, with a focus on laser powder bed fusion (LPBF). Due to the broad range of potential candidate alloys, ORNL and INL focused on Ni-based alloys, while ANL and PNNL mainly evaluated Fe-based alloys. PNNL previously published materials scorecards reports on several key alloys and this report is providing a broader overview of Ni-based candidate alloys, expending beyond alloys well-known to the nuclear community. Of particular interest are alloys that are currently commercially available in powder form due to the growing demand from other industries that have invested heavily in additive manufacturing. Among these alloys, Haynes 282 (Fe-20Cr-20Co-8Mo) was selected due to its superior strength at high temperature compared to the code-qualified alloy 617 (Ni-20-24Cr-10-15Co-8-10Mo). To assess the integration of this new alloy into the AMMT digital manufacturing framework, we performed the rapid optimization of alloy 282 printing parameters on a Renishaw 250 machine, the fabrication of sufficient materials for extensive characterization and mechanical testing both at ORNL and INL, and added the printing data into the digital platform via the Peregrine software. A detailed analysis of the LPBF 718 alloy was also conducted, with creep specimens being tested at 600-650°C and characterized by advanced electron microscopy. The alloy superior mechanical strength and great printability associated with the extensive database that has already been generated highlight the promising potential of LPBF 718 as a candidate alloy for the AMMT program. INL, ANL and PNNL have generated similar reports and all the information will be compiled into a final M2 milestone report to provide the AMMT leadership team with clear recommendations on the down selection of reactor materials, as well as establish a roadmap for the qualification of these selected alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2018

High-temperature deformation behavior of the extruded Ti-22Al-25Nb alloy fabricated by powder metallurgy

Highlights: • The high-temperature deformation behavior of the extruded Ti-22Al-25Nb alloy was analyzed. • A true strain-compensated Arrhenius-type constitutive model was established. • The processing maps of true strains 0.2, 0.4, and 0.6 were constructed to optimize the processing parameters. • Microstructural evolution and deformation mechanism in different conditions were explained. - Abstract: The hot-deformation behavior of the extruded Ti-22Al-25Nb alloy was investigated by compression testing in the 1213–1333 K temperature range, under a 0.001–1.0 s{sup −1} strain-rate range. The activation energy, Q, at a deformation strain of 0.3, was calculated to be 574.80 kJ mol{sup −1}. A strain-compensated Arrhenius-type constitutive model was established for this alloy, with an average absolute relative error (AARE) and correlation coefficient (R) of 7.64% and 0.994, respectively. Based on the dynamic materials model (DMM), processing maps were developed by combining the power dissipation and instability maps. An instability region was identified in the 1213–1278 K temperature range and 0.022–1.0 s{sup −1} strain-rate range. The microstructure of specimens deformed under different conditions were analyzed to characterize the corresponding deformation mechanisms. The main softening mechanisms in the stability regions were dynamic recrystallization (DRX) and dynamic globularization. The grain size of the specimen deformed at 1313 K/0.001 s{sup −1} was approximately 15.2 μm.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Quantitative Evaluations of Surface Cleanliness in IF Steel Slabs at Unsteady Casting

Macro-inclusions in the surface layer of slabs are mainly responsible for the sliver defects in IF steel sheets. In the present work, macro-inclusions in six kinds of unsteady cast IF steel slabs involving four unsteady states (casting start, ladle change, nozzle change and casting end) in one casting sequence were quantitatively characterized using an automatic inclusion analyzer with a total detection area of 238,048 mm{sup 2}. The cleanliness of corresponding normal slabs was also evaluated as the benchmark study, and the number density (ND) of inclusions > 50 µm was used to describe the surface slab cleanliness. Generally, alumina-based and mold powder inclusions were detected, and the former type was further subdivided into alumina clusters, alumina associated with bubbles, refractory-related alumina, Al-Ti complex oxides and CaO-Al{sub 2}O{sub 3}-MgO. Several large-sized alumina-based inclusions were detected in the normal slabs with an average ND of 0.31 N/cm{sup 2}, although they had very low total oxygen (TO) contents (10~13 ppm). No mold powder inclusions were found in normal slabs. For all the unsteady slabs, alumina-based and mold powder inclusions were both observed, and the percentage of the former kind was ≥ 90 pct. The average density of macro-inclusions for the first slab was 1.621 N/cm{sup 2}, whose cleanliness was much worse than any of the other unsteady slabs. The first slab should be downgraded. For the second slab, the ND of macro-inclusions was 0.385 N/cm{sup 2}, which was still larger than the normal slabs because of the lasting effect of the re-oxidation. For the penultimate, cap-off and SEN changed slabs, the density of macro-inclusions fluctuated from 0.25~0.35 N/cm{sup 2}, which was close to the average level of normal slabs. However, mold flux-originated inclusions were frequently observed in these slabs because of flow pattern variations due to the casting speed change. In terms of the slab during the ladle change process, mold powder inclusions were frequently detected even though the casting speed remained constant. A mold powder entrapment mechanism was proposed, which showed the entrapment occurred owing to the flow pattern change induced by forming/dropping of SEN clogs due to re-oxidation by FeO in the ladle slag and tundish steel temperature variations during the ladle change practice. The severity of powder entrapment and re-oxidation was also given for different kinds of unsteady slabs, which provides a direct guide to treating these slabs in the steel plant.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Characterization of Properties for a Gamma–Irradiated ‘Revised’ International Simple Glass

Simplified surrogate high-level waste glasses from recent national and international testing were irradiated to gamma doses of 100 Mrad and 200 Mrad. Properties of the irradiated glass were measured for comparison to the pristine unirradiated glass. Glass transition temperatures as well as infrared and Raman spectroscopy measurements show no change in the irradiated glass. Short-term aqueous corrosion tests on the glass powders also indicate no measurable differences comparing the irradiated to pristine samples. Some corrosion differences were observed in the pristine glasses due to slight compositional changes. As expected from the observed radiation darkening of the glass, absorbance spectra of the irradiated glass with the pristine glass used as LDRD–2021–00341 LDRD External Report Summary reference indicates a broad absorbance over the range of 400 to 700 nm that is centered around 550-600 nm.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

Five new ternary indium-arsenides discovered. Synthesis and structural characterization of the Zintl phases Sr 3 In 2 As 4 , Ba 3 In 2 As 4 , Eu 3 In 2 As 4 , Sr 5 In 2 As 6 and Eu 5 In 2 As 6

Five new ternary indium aresenides, AE 3 In 2 As 4 ( AE =Sr, Ba, Eu), and AE 5 In 2 As 6 ( AE =Sr, Eu), have been synthesized using molten metal In, Pb, and Sn fluxes. Structure elucidation was aided by powder X-ray and single crystal X-ray diffraction. This demonstrated Sr 3 In 2 As 4 and Eu 3 In 2 As 4 are orthorhombic and isostructural to Sr 3 In 2 P 4 (space group Pnnm , Z =2), while Ba 3 In 2 As 4 is monoclinic and isostructural to Ca 3 Al 2 As 4 (space group C 2/ c , Z =4). In addition, Sr 5 In 2 As 6 and Eu 5 In 2 As 6 crystallize orthorhombically and adopt the Ca 5 Ga 2 As 6 structure type (space group Pbam , Z =2). The valence electron count for all structures conform to the Zintl-Klemm concept, and as such can be rationalized as divalent Sr, Ba, Eu cations and polyanionic In–As fragments of different dimensionality. In Sr 3 In 2 As 4 and Eu 3 In 2 As 4 , one-dimensional chains [In 2 As 4 ] 6– running along the crystallographic c -axis exist, and they are made up of edge- and corner-shared tetrahedra InAs 4 . The [In 2 As 4 ] 6– two-dimensional sheets in the structure of Ba 3 In 2 As 4 are composed of a pair of edge-shared InAs 4 tetrahedra, that are further connected by corner-sharing. In Sr 5 In 2 As 6 and Eu 5 In 2 As 6 , the InAs 4 tetrahedra are only corner-shared to make infinite [InAs 2 As 2/2 ] 6– chains running along the a -axis, which are dimerized via As–As bonds into [In 2 As 6 ] 10- ribbons. Furthermore, electronic structure calculations affirm these assignments and suggest intrinsic, narrow-gap seminconducting behavior.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Quantifying the Impact of Metal Population Distribution in MFI-Supported Mo Catalysts for Methane Dehydroaromatization

Precise evaluation of intrinsic kinetic behavior in Mo/MFI catalysts for methane dehydroaromatization (MDA) is confounded by variations in Mo dispersion and speciation, which are influenced by metal loading and zeolite acidity. This work advances the utility of H 2 -temperature programmed reduction (H 2 -TPR) for characterizing Mo/MFI catalysts by enabling quantitative comparison of MoO x populations distinguished by reduction behavior and linked to initial catalytic performance. A comprehensive H 2 reduction pathway is established through systematic H 2 - TPR studies varying catalyst composition (1–10 wt % Mo, Si/Al = 15, 40, ∞), supplemented by UV-Raman spectroscopy, X-ray powder diffraction, N 2 physisorption, NH 3 -TPD, and advanced spectroscopic analysis (in situ XAS with principal component analysis/multivariate curve resolution—alternating least squares). Two low-temperature H 2 -TPR regions capture distinct Mo populations undergoing initial Mo(VI)→Mo(IV) reduction: a lower-temperature population (Mo-RI) associated primarily with highly dispersed, anchored MoO x species expected to predominantly reside within MFI channels, and a higher-temperature population (Mo-RII) corresponding to a broader set of MoO x species that becomes increasingly bulk-like/extrazeolitic at higher Mo loading. Quantification of these populations provides practical, kinetically relevant descriptors for comparing initial MDA rates across catalysts with varying Mo loading, Si/Al ratio, and MoO x heterogeneity. Application of lower-temperature Mo-RI estimates to kinetic measurements reveals a minimum threshold of ∼0.12 × 10 –3 mol Mo-RI/g cat , above which initial forward benzene rates normalized to this population converge despite differences in metal loading and zeolite Brønsted acidity. This threshold coincides with a transition toward a common C 2 -mediated benzene-forming regime, as indicated by approach-to-equilibrium analysis of methane-to-ethane, ethane-to-ethylene, and ethylene-to-benzene reaction steps. Above this threshold, normalized initial benzene rates are nearly invariant with increasing Mo-RII/Mo-RI population ratio, indicating that excess Mo-RII populations, including bulk-like/extrazeolitic MoO x domains present at higher loading, do not measurably suppress benzene formation associated with anchored and mostly channel-confined Mo population under the initial-rate conditions examined.

Mo/MFI↗
DOE OSTI2026

3D printed water-stable Cd-doped Cs 4 MnBi 2 Cl 12 /polylactic acid perovskite/polymer composites for high-flux X-ray scintillation

Stable and efficient X-ray scintillators are crucial for medical diagnostics, industrial, and defense applications. However, conventional scintillator technologies face a trade-off between stability, optimal performance, and sustainability. Herein, we introduce 3D-printed Cs 4 MnBi 2 Cl 12 (Pero1) and Cs 4 Cd 0.68 Mn 0.32 Bi 2 Cl 12 (Pero2) perovskite microcrystals embedded within a polylactic acid (PLA) polymer composite as X-ray scintillators, combining efficiency, stability, and sustainability. The orange luminescent perovskite powder phosphors exhibited poor water stability, which was successfully addressed through incorporation into PLA via filament extrusion and fused deposition modeling (FDM) 3D printing. The resulting composite films demonstrated remarkable water stability while maintaining uniform orange emission throughout the polymer matrix, as confirmed by 3D topography scanning and X-ray fluorescence mapping. Structural characterization revealed minimal chemical interaction between the perovskite and PLA matrix, with the composites retaining their crystalline properties. The PLA-Pero2 composite exhibited superior optical properties, with a photoluminescence quantum yield of 47%, nearly 17 times higher than that of PLA-Pero1 (2.8%), attributed to the effective suppression of non-radiative decay pathways through Cd 2+ doping. Under hard X-ray irradiation at synchrotron beamlines, both composites exhibited excellent radioluminescence, with emission peaks at 605 nm, a linear response across a wide X-ray flux range, and remarkable radiation stability, showing less than 3% intensity degradation after 600 seconds of continuous high-dose exposure. The PLA-Pero2 composite achieved a spatial resolution of 5 line pairs per millimeter and a contrast ratio of 0.255. These performance metrics, combined with the polymer's biodegradability and scalability through additive manufacturing, position PLA-based composites as a more sustainable alternative to conventional petroleum-based polymer scintillators for next-generation medical imaging, radiation monitoring, and industrial radiography applications.

3D Printing↗
DOE OSTI2021

Synthesis and behavior of bulk iron nitride soft magnets via high-pressure spark plasma sintering

Abstract In this study, dense bulk iron nitrides (Fe x N) were synthesized for the first time ever using spark plasma sintering (SPS) of Fe x N powders. The Fe 4 N phase of iron nitride in particular has significant potential to serve as a new soft magnetic material in both transformer and inductor cores and electrical machines. The density of SPSed Fe x N increased with SPS temperature and pressure. The microstructure of the consolidated bulk Fe x N was characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. XRD revealed a primary phase of Fe 4 N with secondary phases of Fe 3 N and metallic iron. Finite element analysis (FEA) was also applied to investigate and explain localized heating and temperature distribution during SPS. The effects of processing on interface bonding formation and phase evolution were investigated and discussed in detail to provide insight into fundamental phenomena and microstructural evolution in SPSed Fe x N. Graphic abstract

36 MATERIALS SCIENCE↗
DOE OSTI2021

The mechanical response of micron-sized molecular crystals

Abstract Microstructures and corresponding properties of compacted powders ultimately depend on the mechanical response of individual particles. In principle, computational simulations can predict the results of powder compaction processes, but the selection of appropriate models for both particle–particle interactions and particle deformations across all relevant length scales remain nontrivial tasks, especially in material systems lacking detailed mechanical property information. The work presented here addresses these issues by conducting uniaxial compressions in situ inside of a scanning electron microscope to characterize the mechanical response of individual micron-sized particles of a molecular crystal, hexanitrohexaazaisowurtzitane (CL-20). This experimental approach enabled the collection of quantitative force and displacement data alongside simultaneous imaging to capture morphology changes. The results reveal information about elastic deformation, yield, plastic deformation, creep, and fracture phenomena. Accordingly, this work demonstrates a generalizable approach for assessing the mechanical response of individual micron-sized molecular crystal particles and utilizing those responses in particle-level models. Graphic abstract

36 MATERIALS SCIENCE↗